CN112305113A - Analysis method of metham sodium - Google Patents
Analysis method of metham sodium Download PDFInfo
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Abstract
A metham analysis method comprises the following steps of preparing a metham standard solution: weighing metham standard substance, dissolving by using methanol + water solution as diluent, adjusting the pH value to 7.5-9.5 by using triethylamine, fixing the volume, and uniformly mixing for later use; preparing a metham sample solution: weighing a metam sample, dissolving the metam sample by using a methanol + water solution as a diluent, adjusting the pH value to 7.5-9.5 by using triethylamine, and performing constant volume and uniform mixing for later use; performing high performance liquid chromatography analysis and determination: adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution and tetrabutyl ammonium bisulfate, the flow rate is 1.0ml/min, the ambient temperature and the column temperature are 15-22 ℃, the detection wavelength is 255-285nm, and the sample injection amount is 5 mu L; and analyzing and measuring the metam standard solution and the metam sample solution by using a high performance liquid chromatography to obtain a metam HPLC chromatogram, and obtaining the metam content according to a liquid chromatography external standard method. The analysis method is simple, convenient and quick, has high accuracy and precision, and can reduce the damage to human bodies and the environment.
Description
Technical Field
The invention relates to the technical field of pesticide analysis, in particular to a metam-sodium analysis method.
Background
Metam sodium, the chemical name of which is sodium methyldithiocarbamate, is a white powder which is easy to absorb moisture, and the industrial product is a light yellow to amber liquid which is dissolved in methanol and water but not dissolved in most organic solvents, and is decomposed by acid and heavy metal salt, but plays a good role in fumigating soil. The acute oral LD50 of the rat is 285-1800mg/kg, and is nontoxic to bees.
Metam is a soil disinfectant with fumigation effect, is suitable for nematode prevention and control of other root crops such as peanuts, cotton, strawberries, gingers and the like, and has killing effect on weeds and grass seeds within one year. In moist soil, within two weeks of metam. Ion chromatography and chemical detection methods are reported in the literature. And (3) analyzing by adopting a chemical method, releasing carbon disulfide from a sample by acid, absorbing by using a potassium hydroxide-methanol solution to generate potassium xanthate, titrating by using iodine, and substituting the coefficient into the calculation. The method has many disadvantages, the first method uses a large amount of chemical reagents, needs heating to release hydrogen sulfide gas, does not completely collect hydrogen sulfide gas, causes a lot of damage to human bodies, and the second method has the disadvantages of complex operation, long time consumption, poor accuracy and low precision recovery rate: the reproducibility of the sample measured by the ion chromatography is poor, and the operability is not strong. By adopting ion chromatography, since metham belongs to an alkaline substance, the corrosion to a chromatographic column is caused, the service life is short, and the analysis cost is high; and the method can not completely elute and separate the metham sample.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a metam content analysis method, which adopts High Performance Liquid Chromatography (HPLC) to analyze the metam content, not only improves the separation effect, but also reduces the zero harm of environmental pollution to human bodies, and can obtain satisfactory results on accuracy and precision.
In order to achieve the purpose, the metam analysis method comprises the following steps:
preparing a metham standard solution: weighing metham standard substance, dissolving by using methanol + water solution as diluent, adjusting the pH value to 7.5-9.5 by using triethylamine, fixing the volume, and uniformly mixing for later use;
preparing a metham sample solution: weighing a metam sample, dissolving the metam sample by using a methanol + water solution as a diluent, adjusting the pH value to 7.5-9.5 by using triethylamine, and performing constant volume and uniform mixing for later use;
performing high performance liquid chromatography analysis and determination: adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution and tetrabutyl ammonium bisulfate, the flow rate is 1.0ml/min, the ambient temperature and the column temperature are 15-22 ℃, the detection wavelength is 255-285nm, and the sample injection amount is 5 mu L; and analyzing and measuring the metam standard solution and the metam sample solution by using a high performance liquid chromatography to obtain a metam HPLC chromatogram, and obtaining the metam content according to a liquid chromatography external standard method.
Further, the volume ratio of the methanol + water solution is 30: 70; the content of the tetrabutylammonium bisulfate is 1 g/L.
Further, the step of analyzing and measuring the metam standard solution by high performance liquid chromatography further comprises the step of repeatedly feeding samples until the difference between peak areas obtained by two adjacent samples is less than 1%.
Further, performing high performance liquid chromatography analysis and determination according to the sequence of the metham standard solution, the metham sample solution and the metham standard solution to obtain the metham HPLC chromatogram.
Furthermore, the metham content is obtained according to a liquid chromatography external standard method, and is calculated according to a liquid chromatography external standard method formula:
wherein:
a1 represents the area of the generation peak in the standard solution;
a2 denotes the area of the generation peak in the sample solution;
m1 represents the standard quality;
m2 represents the sample mass;
p represents the standard quality percentage;
x represents the percentage of metham in the sample.
Compared with the prior art, the metam analysis method has the following technical effects:
1. the mobile phase and the diluted sample are carried out under the alkaline condition, so that the metam is prevented from being decomposed when encountering acid;
2. a large amount of toxic and harmful chemical reagents in a chemical method are abandoned, so that the method is green, environment-friendly, quick, efficient and intelligent, and has no harm to human bodies and the environment;
3. the accuracy is high: the average recovery rate is 99.23%, and the precision draft is as follows: the standard deviation is 0.14%, and the coefficient of variation is 0.41;
4. the deviation is small: the deviations were all within 0.42%.
5. High-value chemical reagents such as iodine, potassium iodide, EDTA and cadmium sulfate are used in the chemical analysis, the analysis time is 90 minutes, and a large amount of labor is consumed; by adopting the analysis method, only a small amount of methanol and all the other methanol are used, the analysis time is only 10 minutes, and a large amount of chemical reagents and labor force are saved.
Drawings
Figure 1 is an HPLC chromatogram of a metam standard according to the invention;
figure 2 is an HPLC chromatogram of a metam sample according to the invention;
figure 3 is a metam standard curve according to the present invention.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
In order to better explain the present invention, the present invention is further explained below with reference to specific examples. The apparatus used in the following examples was: the liquid chromatograph is provided with an ultraviolet detector and an automatic sample introduction system; the chromatographic column is as follows: (C18) 250X 4.6(pH 2-10); the sample injector is as follows: 5 μ L sample injector. The metam standard described in the examples was 85.0 wt% metam, and other materials and agents, such as those available commercially without specific indication, were available.
In the embodiment of the invention, the diluted solution is a solution (pH7.5-9.5) of methanol + water which is 30+ 70; the mobile phase is as follows: methanol: water ═ 30+70) +1g/l tetrabutylammonium hydrogen sulfate (pH7.5-9.5)
Example 1
Preparing a metham standard solution: accurately weighing 40mg (accurate to 0.01mg) of the metam standard substance with the content of 85.0 wt%, diluting the metam standard substance in a 100ml volumetric flask with a methanol + aqueous solution (the volume ratio of methanol to water is 30:70), and uniformly shaking the solution by ultrasonic waves for later use, wherein the HPLC chromatogram of the metam standard substance is shown in figure 1.
Preparing a metham sample solution: about 40mg (accurate to 0.01mg) of a metam sample is accurately weighed into a 100ml volumetric flask, diluted by a methanol + water solution (the volume ratio of methanol to water is 30:70), and uniformly shaken by ultrasound for later use, and the HPLC chromatogram of the metam sample is shown in figure 2.
Example 2
Metam standard solution and metam sample solution were prepared according to the method of example 1
Adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution (the volume ratio of methanol to water is 30:70) and 1g/L tetrabutylammonium bisulfate, the flow rate is 1.0ml/min, the column temperature is 22 ℃, the detection wavelength is 255nm, and the sample injection amount is 5 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is less than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to a liquid chromatography external standard method formula, the metham content is 35.07%.
Example 3
Metam standard solutions and metam sample solutions were prepared according to the method of example 1.
Adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution (the volume ratio of methanol to water is 30:70) and 1g/L tetrabutylammonium bisulfate, the flow rate is 1.0ml/min, the column temperature is 20 ℃, the detection wavelength is 255nm, and the sample injection amount is 5 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is less than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to an external standard method formula of liquid chromatography, the metham content is 35.33%.
Example 4
Metam standard solutions and metam sample solutions were prepared according to the method of example 1.
Adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution (the volume ratio of methanol to water is 30:70) and 1g/L tetrabutylammonium bisulfate, the flow rate is 1.0ml/min, the column temperature is 16 ℃, the detection wavelength is 255nm, and the sample injection amount is 5 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is more than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to a liquid chromatography external standard method formula, the metham content is 35.19%.
Example 5
Metam standard solutions and metam sample solutions were prepared according to the method of example 1.
Adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution (the volume ratio of methanol to water is 30:70) and 1g/L tetrabutylammonium bisulfate, the flow rate is 1.0ml/min, the column temperature is 22 ℃, the detection wavelength is 280nm, and the sample injection amount is 5 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is less than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to a liquid chromatography external standard method formula, the metham content is 35.22%.
Example 6
Metam standard solutions and metam sample solutions were prepared according to the method of example 1.
A C18 chromatographic column is adopted, and the mobile phases are methanol + water solution (the volume ratio of methanol to water is 30:70) and 1g/L tetrabutyl ammonium bisulfate methanol: the flow rate is 1.0ml/min, the column temperature is 22 ℃, the detection wavelength is 279nm, and the sample injection amount is 5 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is more than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to a liquid chromatography external standard method formula, the metham content is 35.64%.
Example 7
Metam standard solutions and metam sample solutions were prepared according to the method of example 1.
Adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution (the volume ratio of methanol to water is 30:70) and 1g/L tetrabutyl ammonium bisulfate methanol, the flow rate is 1.0ml/min, the column temperature is 22 ℃, the detection wavelength is 269nm, and the sample injection amount is 5 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is less than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to a liquid chromatography external standard method formula, the metham content is 35.97%.
Example 8
Metam standard solutions and metam sample solutions were prepared according to the method of example 1.
A C18 chromatographic column was used, and the ratio of methanol + aqueous solution (methanol to water volume ratio: 30:70) and 1g/L of tetrabutylammonium bisulfate methanol: the flow rate is 0.6ml/min, the column temperature is 22 ℃, the detection wavelength is 280nm, and the sample injection amount is 20 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is less than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to a liquid chromatography external standard method formula, the metham content is 35.99%.
Example 9
Metam standard solutions and metam sample solutions were prepared according to the method of example 1.
A C18 chromatographic column was used, and the ratio of methanol + aqueous solution (methanol to water volume ratio: 30:70) and 1g/L of tetrabutylammonium bisulfate methanol: the flow rate is 0.9ml/min, the column temperature is 22 ℃, the detection wavelength is 280nm, and the sample injection amount is 5 mu L; introducing the sample into a standard solution under the conditions, repeatedly introducing the sample until the difference between peak areas obtained by two adjacent times of sample introduction is less than 1%, and then performing HPLC analysis according to the sequence of the standard, the sample and the standard to obtain a metam HPLC chromatogram; according to an external standard method formula of liquid chromatography, the metham content is 35.33%.
In the embodiment of the invention, the formula of the liquid chromatography external standard method for calculating the metham content in the sample is as follows:
wherein:
a1 represents the area of the generation peak in the standard solution;
a2 denotes the area of the generation peak in the sample solution;
m1 represents standard mass (mg);
m2 represents sample mass (mg);
p represents percent (%) standard quality;
x represents the percentage of metham in the sample.
The following are examples of the present invention for analyzing the metham content
Example 10 Standard Curve
Metam standard substances with different masses are respectively weighed, the metam standard substance solutions with the concentrations of 264.6mg/L, 352.9mg/L, 441.0mg/L, 538.2mg/L and 618.2mg/L are prepared according to the method for preparing the standard substance solution in the example 1, sample injection is carried out according to the chromatographic conditions in the example 2, the peak areas are measured, and the measurement results are shown in the table 1.
TABLE 1 metam quantitative analysis Linear Range assay
Drawing a standard curve by taking the weighed sample as an abscissa and the peak area as an ordinate to obtain a regression equation of which Y is 22.5267X +11.8004 and a correlation coefficient R2The standard curve of 0.9994 and 0.9997 is shown in fig. 3.
EXAMPLE 11 precision test
Separately weighing metham samples (batch: 202001015-2) with different masses, preparing metham sample solutions according to the method for preparing the sample solutions in the embodiment 1 and the chromatographic conditions same as those in the embodiment 2, injecting and detecting the samples, measuring peak areas, and calculating the metham content in each sample, wherein the results are shown in table 2.
TABLE 2 metam quantitative analysis precision measurement results
The results in table 2 show that the standard deviation of the obtained metham content is 0.14% and the coefficient of variation is 0.41.
Example 12 accuracy experiment
Metham standard substances with different amounts are respectively added into metham raw drug to prepare samples with known content, the samples are injected and detected, the peak area is measured, and the results of the recovery rate calculation are shown in table 3 according to the measurement of example 1.
TABLE 3 metam quantitative analysis accuracy determination results
The results in table 3 show that the average recovery of the metam standard was 99.23%, indicating that the accuracy of analysis of metam content using hplc was high.
Example 13
The content of metham in the metham sample was analyzed using the HPLC assay method of the present invention (according to the chromatographic conditions of example 2) and the chemical assay method, respectively, and the results are shown in table 4.
TABLE 4 Weibaimu content obtained by different analytical methods
| Batch number | 112-1 | 113-2 | 114-1 | 114-2 | 117-2 |
| Chemical analysis content% | 35.42 | 34.85 | 34.90 | 35.60 | 35.36 |
| Content of instrument analysis% | 35.24 | 34.96 | 35.32 | 35.19 | 35.06 |
| Deviation% | -0.18 | +0.11 | +0.42 | -0.41 | -0.30 |
The results in table 4 show that the deviation of the HPLC assay and chemical assay methods of the invention to metam content was in the range of 0.5%.
Those of ordinary skill in the art will understand that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A metham analysis method comprises the following steps:
preparing a metham standard solution: weighing metham standard substance, dissolving by using methanol + water solution as diluent, adjusting the pH value to 7.5-9.5 by using triethylamine, fixing the volume, and uniformly mixing for later use;
preparing a metham sample solution: weighing a metam sample, dissolving the metam sample by using a methanol + water solution as a diluent, adjusting the pH value to 7.5-9.5 by using triethylamine, and performing constant volume and uniform mixing for later use;
performing high performance liquid chromatography analysis and determination: adopting a C18 chromatographic column, wherein the mobile phase comprises methanol + water solution and tetrabutyl ammonium bisulfate, the flow rate is 1.0ml/min, the ambient temperature and the column temperature are 15-22 ℃, the detection wavelength is 255-285nm, and the sample injection amount is 5 mu L; and analyzing and measuring the metam standard solution and the metam sample solution by using a high performance liquid chromatography to obtain a metam HPLC chromatogram, and obtaining the metam content according to a liquid chromatography external standard method.
2. A metam-sodium analysis method according to claim 1 wherein the volume ratio of the methanol + aqueous solution is 30: 70; the content of the tetrabutylammonium bisulfate is 1 g/L.
3. The metam-sodium analysis method according to claim 1, wherein the step of performing high performance liquid chromatography analysis and measurement on the metam-sodium standard solution further comprises repeating the sample injection until the difference between peak areas obtained by two adjacent sample injections is less than 1%.
4. The metam-sodium analysis method according to claim 1, further comprising performing high performance liquid chromatography analysis and determination according to the sequence of metam standard solution, metam sample solution and metam standard solution to obtain metam HPLC chromatogram.
5. The metam-sodium analysis method according to claim 1, wherein the metam-sodium content is obtained according to a liquid chromatography external standard method, and is calculated in a sample according to the following liquid chromatography external standard method formula:
wherein:
a1 represents the area of the generation peak in the standard solution;
a2 denotes the area of the generation peak in the sample solution;
m1 represents the standard quality;
m2 represents the sample mass;
p represents the standard quality percentage;
x represents the percentage of metham in the sample.
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| CN117805278A (en) * | 2023-12-30 | 2024-04-02 | 上海新泊地化工技术服务有限公司 | Method for analyzing short-chain organic acid in soldering flux by liquid chromatography |
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| CN117805278A (en) * | 2023-12-30 | 2024-04-02 | 上海新泊地化工技术服务有限公司 | Method for analyzing short-chain organic acid in soldering flux by liquid chromatography |
| CN117805278B (en) * | 2023-12-30 | 2024-05-17 | 上海新泊地化工技术服务有限公司 | Method for analyzing short-chain organic acid in soldering flux by liquid chromatography |
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